CN105086502A - Novel nanometer titania/chlorophyll derivative dye and preparation method thereof - Google Patents
Novel nanometer titania/chlorophyll derivative dye and preparation method thereof Download PDFInfo
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- CN105086502A CN105086502A CN201510565522.0A CN201510565522A CN105086502A CN 105086502 A CN105086502 A CN 105086502A CN 201510565522 A CN201510565522 A CN 201510565522A CN 105086502 A CN105086502 A CN 105086502A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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Abstract
The invention provides a novel nanometer titania/chlorophyll derivative dye and a preparation method thereof. The preparation method comprises the following steps: cleaning and drying leaf stems of fresh plant; processing the leaf stems with a cupric sulfate solution to obtain a chlorophyll-stable plant raw material; then preparing the pre-treated plant raw material into plant powder; adding the plant powder into ethanol water; performing light-proof sealing and stirring; conducting ultrasonic oscillation; filtering and taking the filtrate; concentrating the filtrate to obtain a chlorophyll extracting solution; adding a sodium hydroxide and ethanol solution into the chlorophyll extracting solution to saponify chlorophyll; adding a sulfate solution; adding water for dilution; filtering to obtain a solid chlorophyll derivative; finally, dissolving the solid chlorophyll derivative into ethanol water; performing quick stirring; adding a nanometer titania solution dropwise; performing intensive stirring to obtain the nanometer titania/chlorophyll derivative dye. The prepared dye is high in absorbency, good in stability, high in water solubility and excellent in color fastness, and a fabric dyed by the dye is bright and long-lasting in color and high in wash resistance and light fastness.
Description
Technical field:
The invention belongs to textile materials technical field, be specifically related to the dye well its preparation method of a kind of novel nano titanium dioxide/phyllins.
Background technology:
Natural dyestuff refers to from plant, animal, obtain in microorganism or Mineral resources, seldom or not through the dyestuff of chemical process, China is one of country using natural dyestuff the earliest, although since synthetic dyestuff are born, because synthetic dyestuff chromatogram is complete, bright in colour, washable sun-proof, the reasons such as low price, natural dyestuff is replaced gradually, but along with people are in recent years to the pay attention to day by day of environmental protection and self health care, the easy skin irritation of many synthetic dyestuff, cause the diseases such as tetter, the fabric shade of natural dye dying is unique unique, individual character is various, but also have part nourishing function concurrently, therefore nontoxic free of contamination natural dyestuff is valued by the people again gradually.
One of natural dye dying subject matter is exactly Fastness Problems, the ecological criteria of dyed textiles and the dyefastness of dyestuff have relation closely, although can dyefastness be improved by mordant dyeing and aftertreatment technology at present, but because natural dyestuff chromophoric group inherent instability, therefore not still very good for the finishing effect that natural dyestuff is washable and fast light, and usually all contain heavy metal ion in the mordant adopted, not only destroy the green of natural dyestuff, even also can affect the color and luster of finished product.Therefore set about improving from the chromophoric group of natural dyeing the Fastness Problems that the washable of natural dyestuff and photostabilization fundamentally could solve natural dyestuff.
The pigment of natural dyestuff can be divided into according to chemical structure and character: carotenoids, flavonoid class, chlorophyll class, Polyphenols, quinones, diones, indoles, alkaloids and other plant pigment, wherein, chlorophyll is a kind of green pigment be present in leaf, stem, it structure is coloured heterogeneous ring compound of porphyrin, dissolve in alcohols material, and chlorophyll can present the color such as green, brown according to different process gimmicks.
The disclosed method improving sodium copper chlorophyllin dyeing cotton fabric sunlight fastness of Chinese patent CN102251413B (publication date 2011.11.23), by before dyeing, dyeing time or dyeing after add the natural sophora bud, on the natural sophora bud with hydroxyl can and cellulosic fabric between form hydrogen bond, and the natural sophora bud has good uvioresistant ability, what can absorb in daylight is UV protection, therefore add the colour fastness that the sophora bud comprehensively can improve dyestuff, reduce fading of DYED FABRICS.The disclosed a kind of chlorophyll of Chinese patent CN103485196B (publication date 2014.1.1) is to the dyeing of modified fabric, with the polyester/cotton blended fabric dyeing of natural dyestuff chlorophyll to cation modifying, improve the tinting strength of dyestuff, improve the colour fastness of fabric, and environment is not polluted.From above-mentioned prior art, can by fabric-modifying or add the colour fastness that auxiliary agent improves fabric in dyestuff, but group modifiedly improve its dyeability from chlorophyllous, research is few at present.
Summary of the invention:
The technical problem to be solved in the present invention is to provide the dye well its preparation method of a kind of novel nano titanium dioxide/phyllins, adopt nano titanic oxide sol and leaf green derivative as main raw material, after proportioning, obtain the dyestuff of nano titanium oxide/phyllins.The absorbancy of the dyestuff of nano titanium oxide/phyllins prepared by the present invention is high, good stability, and greatly water-soluble, colour fastness is good, through fabric lastingly bright-colored of this dyeing, water-fastness and weathering color fastness is high.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for the dyestuff of novel nano titanium dioxide/phyllins, is characterized in that: comprise the following steps:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 1-2mol/L soaks 30-50min, and take out, thoroughly wash away unnecessary copper sulfate with clear water, drying in the shade under room temperature obtains pretreated plant material;
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into plant powder, plant powder is added the aqueous ethanolic solution of 80-100%, 30min is stirred in shading sealing, ultra-sonic oscillation 30-50min, cross leaching filtrate, concentrate and obtain chlorophyll extracting solution;
(3) by weight, the sodium hydroxide ethanolic soln of the 3-5% of 10-20 part is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 55-65 DEG C of heated and stirred makes chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add the sulfate liquor of 35-45 part, thin up, filters and obtains phyllins solid;
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 8-10 part being dissolved in 10-15 part forms solution A, the dehydrated alcohol deionized water of 2-3 part being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains nano titanic oxide sol;
(5) phyllins solid prepared by step (3) is dissolved in aqueous ethanolic solution, rapid stirring, then dropwise add nano titanic oxide sol prepared by step (4), fully stir the dyestuff obtaining nano titanium oxide/phyllins.
Preferred as technique scheme, in described step (1), the water ratio of pretreated plant material is lower than 5%.
Preferred as technique scheme, in described step (2), the particle diameter of plant powder is micro/nano level.
Preferred as technique scheme, in described step (2), the mass ratio of plant powder and aqueous ethanolic solution is 1:8-12.
Preferred as technique scheme, in described step (2), the solid holdup of chlorophyll extracting solution is 65-80%.
Preferred as technique scheme, in described step (3), sulfate liquor is copper sulfate or the solution of zinc sulfate of 3-6%.
Preferred as technique scheme, in described step (4), in nano titanic oxide sol, the particle diameter of nano titanium oxide is 20-50nm.
Preferred as technique scheme, in described step (5), each component in the dyestuff of nano titanium oxide/phyllins, by weight, comprising: phyllins solid 45-60 part, ethanol water 90-100 part, nano titanic oxide sol 25-35 part.
The present invention also provides the dyestuff of a kind of nano titanium oxide/phyllins, it is characterized in that, the main raw material of the dyestuff of nano titanium oxide/phyllins is nano titanium oxide and phyllins, described nano titanium oxide is nano titanic oxide sol, and described phyllins are chlorophyll metal-salt.
Preferably, the dyestuff of nano titanium oxide/phyllins is 549-597 at the maximum absorbance of 405-630nm.
Compared with prior art, the present invention has following beneficial effect:
(1) phyllins are contained in the chlorophyll dyestuff that prepared by the present invention, belong to cationic dyes, chlorophyll is carried out the coloured heterogeneous ring compound for porphyrin in modification acquisition phyllins structure, containing strong hydrogen bond, hydrogen bond that can be stable with the intermolecular formation of fabric, improves the colour fastness of chlorophyll dyestuff.
(2) contain nano titanium oxide in the chlorophyll dyestuff that prepared by the present invention, nano titanium oxide has very strong anti-ultraviolet property, and combine with chlorophyll the chlorophyllous dye uptake of this raising tender, improves the colour fastness of chlorophyll dyestuff.
(3) phyllins contained in the chlorophyll dyestuff that prepared by the present invention, that metal ion is replaced magnesium ion again by chlorophyll after saponification reaction, obtain water-soluble large and phyllins that stability is strong, the colour fastness of chlorophyll dyestuff can be significantly improved.
(4) absorbance of the dyestuff of nano titanium oxide/phyllins prepared of the present invention is high, bright-colored, and the colour fastness grade of the fabric after changing dyeing significantly improves, and what meet fabric takes standard.
Embodiment:
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 1mol/L soaks 30min, take out, thoroughly wash away unnecessary copper sulfate with clear water, dry in the shade under room temperature obtain water ratio lower than 5% pretreated plant material.
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into micro/nano level plant powder, by weight, the plant powder of 1 part is added the aqueous ethanolic solution of 8 parts 80%, 30min is stirred in shading sealing, ultra-sonic oscillation 30min, cross leaching filtrate, concentrate and obtain the chlorophyll extracting solution that solid holdup is 65%.
(3) by weight, the sodium hydroxide ethanolic soln of 10 parts 3% is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 55 DEG C of heated and stirred make chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add copper sulfate or the solution of zinc sulfate of 35 parts 3%, thin up, filters and obtains phyllins solid.
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 8 parts being dissolved in 10 parts forms solution A, the dehydrated alcohol deionized water of 2 parts being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains the nano titanic oxide sol of 20-50nm.
(5) by weight, phyllins solid prepared by the steps of 45 parts (3) is dissolved in the aqueous ethanolic solution of 90 parts, rapid stirring, nano titanic oxide sol prepared by the step (4) then dropwise adding 25 parts, fully stirs the dyestuff obtaining nano titanium oxide/phyllins.
Embodiment 2:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 2mol/L soaks 50min, take out, thoroughly wash away unnecessary copper sulfate with clear water, dry in the shade under room temperature obtain water ratio lower than 5% pretreated plant material.
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into micro/nano level plant powder, by weight, the plant powder of 1 part is added the aqueous ethanolic solution of 12 parts 100%, 30min is stirred in shading sealing, ultra-sonic oscillation 50min, cross leaching filtrate, concentrate and obtain the chlorophyll extracting solution that solid holdup is 80%.
(3) by weight, the sodium hydroxide ethanolic soln of 20 parts 5% is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 65 DEG C of heated and stirred make chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add copper sulfate or the solution of zinc sulfate of 45 parts 6%, thin up, filters and obtains phyllins solid.
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 10 parts being dissolved in 15 parts forms solution A, the dehydrated alcohol deionized water of 3 parts being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains the nano titanic oxide sol of 20-50nm.
(5) by weight, phyllins solid prepared by the steps of 60 parts (3) is dissolved in the aqueous ethanolic solution of 100 parts, rapid stirring, nano titanic oxide sol prepared by the step (4) then dropwise adding 35 parts, fully stirs the dyestuff obtaining nano titanium oxide/phyllins.
Embodiment 3:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 1.5mol/L soaks 40min, take out, thoroughly wash away unnecessary copper sulfate with clear water, dry in the shade under room temperature obtain water ratio lower than 5% pretreated plant material.
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into micro/nano level plant powder, by weight, the plant powder of 1 part is added the aqueous ethanolic solution of 10 parts 90%, 30min is stirred in shading sealing, ultra-sonic oscillation 40min, cross leaching filtrate, concentrate and obtain the chlorophyll extracting solution that solid holdup is 70%.
(3) by weight, the sodium hydroxide ethanolic soln of 15 parts 4% is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 60 DEG C of heated and stirred make chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add copper sulfate or the solution of zinc sulfate of 40 parts 5%, thin up, filters and obtains phyllins solid.
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 9 parts being dissolved in 13 parts forms solution A, the dehydrated alcohol deionized water of 2.5 parts being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains the nano titanic oxide sol of 20-50nm.
(5) by weight, phyllins solid prepared by the steps of 50 parts (3) is dissolved in the aqueous ethanolic solution of 95 parts, rapid stirring, nano titanic oxide sol prepared by the step (4) then dropwise adding 30 parts, fully stirs the dyestuff obtaining nano titanium oxide/phyllins.
Embodiment 4:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 1.4mol/L soaks 35min, take out, thoroughly wash away unnecessary copper sulfate with clear water, dry in the shade under room temperature obtain water ratio lower than 5% pretreated plant material.
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into micro/nano level plant powder, by weight, the plant powder of 1 part is added the aqueous ethanolic solution of 10 parts 85%, 30min is stirred in shading sealing, ultra-sonic oscillation 45min, cross leaching filtrate, concentrate and obtain the chlorophyll extracting solution that solid holdup is 70%.
(3) by weight, the sodium hydroxide ethanolic soln of 17 parts 3.5% is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 58 DEG C of heated and stirred make chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add copper sulfate or the solution of zinc sulfate of 41 parts 4%, thin up, filters and obtains phyllins solid.
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 9 parts being dissolved in 13 parts forms solution A, the dehydrated alcohol deionized water of 2 parts being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains the nano titanic oxide sol of 20-50nm.
(5) by weight, phyllins solid prepared by the steps of 55 parts (3) is dissolved in the aqueous ethanolic solution of 96 parts, rapid stirring, nano titanic oxide sol prepared by the step (4) then dropwise adding 28 parts, fully stirs the dyestuff obtaining nano titanium oxide/phyllins.
Embodiment 5:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 1.7mol/L soaks 46min, take out, thoroughly wash away unnecessary copper sulfate with clear water, dry in the shade under room temperature obtain water ratio lower than 5% pretreated plant material.
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into micro/nano level plant powder, by weight, the plant powder of 1 part is added the aqueous ethanolic solution of 11 parts 95%, 30min is stirred in shading sealing, ultra-sonic oscillation 40min, cross leaching filtrate, concentrate and obtain the chlorophyll extracting solution that solid holdup is 75%.
(3) by weight, the sodium hydroxide ethanolic soln of 17 parts 4.5% is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 60 DEG C of heated and stirred make chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add copper sulfate or the solution of zinc sulfate of 38 parts 4.2%, thin up, filters and obtains phyllins solid.
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 9 parts being dissolved in 13 parts forms solution A, the dehydrated alcohol deionized water of 2.8 parts being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains the nano titanic oxide sol of 20-50nm.
(5) by weight, phyllins solid prepared by the steps of 52 parts (3) is dissolved in the aqueous ethanolic solution of 97 parts, rapid stirring, nano titanic oxide sol prepared by the step (4) then dropwise adding 33 parts, fully stirs the dyestuff obtaining nano titanium oxide/phyllins.
Embodiment 6:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 2mol/L soaks 40min, take out, thoroughly wash away unnecessary copper sulfate with clear water, dry in the shade under room temperature obtain water ratio lower than 5% pretreated plant material.
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into micro/nano level plant powder, by weight, the plant powder of 1 part is added the aqueous ethanolic solution of 10 parts 90%, 30min is stirred in shading sealing, ultra-sonic oscillation 40min, cross leaching filtrate, concentrate and obtain the chlorophyll extracting solution that solid holdup is 70%.
(3) by weight, the sodium hydroxide ethanolic soln of 15 parts 3.8% is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 62 DEG C of heated and stirred make chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add copper sulfate or the solution of zinc sulfate of 40 parts 5.5%, thin up, filters and obtains phyllins solid.
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 9 parts being dissolved in 11 parts forms solution A, the dehydrated alcohol deionized water of 3 parts being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains the nano titanic oxide sol of 20-50nm.
(5) by weight, phyllins solid prepared by the steps of 55 parts (3) is dissolved in the aqueous ethanolic solution of 95 parts, rapid stirring, nano titanic oxide sol prepared by the step (4) then dropwise adding 30 parts, fully stirs the dyestuff obtaining nano titanium oxide/phyllins.
After testing, the dyestuff of nano titanium oxide/phyllins prepared of embodiment 1-6 is as follows in the result of the maximum absorbance of 405-630nm:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Maximum absorbance | 549 | 597 | 564 | 581 | 576 | 582 |
After testing, the colour fastness result of the colour fastness of fabric of the dyestuff substantive dyeing of nano titanium oxide/phyllins prepared of embodiment 1-6 and the fabric of common chlorophyll dyestuff substantive dyeing is as follows:
As seen from the above table, the dyeing behavior of the dyestuff of nano titanium oxide/phyllins prepared by the present invention is excellent, and compared with common chlorophyll dyestuff, colour fastness increases significantly.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. a preparation method for the dyestuff of novel nano titanium dioxide/phyllins, is characterized in that: comprise the following steps:
(1) by after the base of leaf clean dry of fresh plant, the copper-bath being placed in 1-2mol/L soaks 30-50min, and take out, thoroughly wash away unnecessary copper sulfate with clear water, drying in the shade under room temperature obtains pretreated plant material;
(2) pretreated plant material prepared by step (1) is cut, shreds, is ground into plant powder, plant powder is added the aqueous ethanolic solution of 80-100%, 30min is stirred in shading sealing, ultra-sonic oscillation 30-50min, cross leaching filtrate, concentrate and obtain chlorophyll extracting solution;
(3) by weight, the sodium hydroxide ethanolic soln of the 3-5% of 10-20 part is added in the chlorophyll extracting solution that the step of 1 part (2) is prepared, 55-65 DEG C of heated and stirred makes chlorophyll saponification, citric acid regulating solution pH value is added to slightly acidic after saponification completely, finally add the sulfate liquor of 35-45 part, thin up, filters and obtains phyllins solid;
(4) under room temperature, count by volume, the dehydrated alcohol butyl (tetra) titanate of the acetic acid of 1 part and 8-10 part being dissolved in 10-15 part forms solution A, the dehydrated alcohol deionized water of 2-3 part being added 10 parts forms B solution, solution B is dropwise added rapid stirring in solution A and obtains nano titanic oxide sol;
(5) phyllins solid prepared by step (3) is dissolved in aqueous ethanolic solution, rapid stirring, then dropwise add nano titanic oxide sol prepared by step (4), fully stir the dyestuff obtaining nano titanium oxide/phyllins.
2. the preparation method of the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 1, is characterized in that: in described step (1), the water ratio of pretreated plant material is lower than 5%.
3. the preparation method of the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 1, is characterized in that: in described step (2), and the particle diameter of plant powder is micro/nano level.
4. the preparation method of the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 1, is characterized in that: in described step (2), and the mass ratio of plant powder and aqueous ethanolic solution is 1:8-12.
5. the preparation method of the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 1, is characterized in that: in described step (2), and the solid holdup of chlorophyll extracting solution is 65-80%.
6. the preparation method of the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 1, is characterized in that: in described step (3), and sulfate liquor is copper sulfate or the solution of zinc sulfate of 3-6%.
7. the preparation method of the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 1, it is characterized in that: in described step (4), in nano titanic oxide sol, the particle diameter of nano titanium oxide is 20-50nm.
8. the preparation method of the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 1, it is characterized in that: in described step (5), each component in the dyestuff of nano titanium oxide/phyllins, by weight, comprising: phyllins solid 45-60 part, ethanol water 90-100 part, nano titanic oxide sol 25-35 part.
9. the dyestuff of novel nano titanium dioxide/phyllins, it is characterized in that, the main raw material of the dyestuff of nano titanium oxide/phyllins is nano titanium oxide and phyllins, described nano titanium oxide is nano titanic oxide sol, and described phyllins are chlorophyll metal-salt.
10. the dyestuff of a kind of novel nano titanium dioxide/phyllins according to claim 9, is characterized in that, the dyestuff of nano titanium oxide/phyllins is 549-597 at the maximum absorbance of 405-630nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108018727A (en) * | 2017-12-27 | 2018-05-11 | 五邑大学 | A kind of preparation method and application of vegetable colour hydridization titanium dioxide water repellent colloidal sol |
| CN109651851A (en) * | 2019-01-15 | 2019-04-19 | 上海崇明木棉花开手工社 | The inorganic-organic hybridization nano pigment and preparation method of natural botanical source and application |
| CN110804289A (en) * | 2019-11-21 | 2020-02-18 | 中华全国供销合作总社济南果品研究院 | Ethylene adsorption nano titanium dioxide polylactic acid film with wide spectral response |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000566A (en) * | 2010-10-15 | 2011-04-06 | 徐志兵 | Method for preparing photoactivated silver/titanium dioxide complex |
| CN102443007A (en) * | 2010-10-15 | 2012-05-09 | 南通玺运贸易有限公司 | Chlorophyll extraction process |
| CN102731513A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting sodium copper chlorophyllin from wild deyeuxia angustifolia forage grass |
| CN103184686A (en) * | 2013-03-20 | 2013-07-03 | 西安工程大学 | Method for modifying and dying wool fiber by tetrabutyl titanate and lanasol dye |
-
2015
- 2015-09-08 CN CN201510565522.0A patent/CN105086502A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000566A (en) * | 2010-10-15 | 2011-04-06 | 徐志兵 | Method for preparing photoactivated silver/titanium dioxide complex |
| CN102443007A (en) * | 2010-10-15 | 2012-05-09 | 南通玺运贸易有限公司 | Chlorophyll extraction process |
| CN102731513A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting sodium copper chlorophyllin from wild deyeuxia angustifolia forage grass |
| CN103184686A (en) * | 2013-03-20 | 2013-07-03 | 西安工程大学 | Method for modifying and dying wool fiber by tetrabutyl titanate and lanasol dye |
Non-Patent Citations (1)
| Title |
|---|
| 郭莉等: "叶绿素铜敏化二氧化钛光催化剂的合成及性能研究", 《江西农业大学学报》 * |
Cited By (4)
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| CN108018727A (en) * | 2017-12-27 | 2018-05-11 | 五邑大学 | A kind of preparation method and application of vegetable colour hydridization titanium dioxide water repellent colloidal sol |
| CN109651851A (en) * | 2019-01-15 | 2019-04-19 | 上海崇明木棉花开手工社 | The inorganic-organic hybridization nano pigment and preparation method of natural botanical source and application |
| CN110804289A (en) * | 2019-11-21 | 2020-02-18 | 中华全国供销合作总社济南果品研究院 | Ethylene adsorption nano titanium dioxide polylactic acid film with wide spectral response |
| CN110804289B (en) * | 2019-11-21 | 2021-10-01 | 中华全国供销合作总社济南果品研究院 | Ethylene adsorption nano titanium dioxide polylactic acid film with wide spectral response |
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